CN117512516A - Preparation method of metal powder surface insulation layer - Google Patents
Preparation method of metal powder surface insulation layer Download PDFInfo
- Publication number
- CN117512516A CN117512516A CN202311566707.4A CN202311566707A CN117512516A CN 117512516 A CN117512516 A CN 117512516A CN 202311566707 A CN202311566707 A CN 202311566707A CN 117512516 A CN117512516 A CN 117512516A
- Authority
- CN
- China
- Prior art keywords
- powder
- target
- temperature
- vacuum
- insulation layer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 97
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 30
- 239000002184 metal Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000009413 insulation Methods 0.000 title claims description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000004544 sputter deposition Methods 0.000 claims abstract description 30
- 229910052786 argon Inorganic materials 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 13
- 238000005086 pumping Methods 0.000 claims abstract description 12
- 238000001755 magnetron sputter deposition Methods 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000012535 impurity Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 7
- 239000007888 film coating Substances 0.000 claims abstract description 6
- 238000009501 film coating Methods 0.000 claims abstract description 6
- 230000005284 excitation Effects 0.000 claims abstract description 4
- 238000001291 vacuum drying Methods 0.000 claims abstract description 4
- 239000011248 coating agent Substances 0.000 claims description 30
- 238000000576 coating method Methods 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 23
- 239000011261 inert gas Substances 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- 238000004321 preservation Methods 0.000 claims description 7
- 238000010301 surface-oxidation reaction Methods 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 230000000630 rising effect Effects 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000013077 target material Substances 0.000 claims description 2
- 239000010410 layer Substances 0.000 description 16
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 239000011247 coating layer Substances 0.000 description 4
- 229910052593 corundum Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 description 4
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000011534 incubation Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000006247 magnetic powder Substances 0.000 description 2
- 238000005240 physical vapour deposition Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000007781 pre-processing Methods 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000007733 ion plating Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/16—Metallic particles coated with a non-metal
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/58—After-treatment
- C23C14/5846—Reactive treatment
- C23C14/5853—Oxidation
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The invention relates to the technical field of metal surface insulating layers, and discloses a preparation method of a metal powder surface insulating layer, which is characterized by comprising the following steps: s1: immersing the powder into ethanol solution for ultrasonic excitation, immersing into deionized water for ultrasonic cleaning, and then placing into a vacuum drying oven for drying treatment; s2: placing the pretreated powder into a coated powder preparation box body, mounting the coated powder on a carrying disc, then mounting a target sputtering source (whether the number is required or not), closing a magnetron sputtering chamber, and starting a vacuum pumping system to perform vacuum extraction; s3: when the vacuum draw reaches the background vacuum of 8.0X10 ‑4 After Pa, opening an argon valve, introducing argon, and then openingA target sputtering power supply for pre-sputtering the target to remove impurities attached to the surface of the target; then the ultrasonic vibration motor is started to carry out film coating on the powder, and after the powder film coating on the conveyor belt is completed.
Description
Technical Field
The invention relates to the technical field of metal surface insulating layers, in particular to a preparation method of a metal powder surface insulating layer.
Background
The metal powder material has good performance and is widely used in various industries, including powder metallurgy, electric carbon products, electronic materials, metal coating, chemical catalysts, filters, radiating pipes and other electromechanical parts, electronic aviation fields and the like. The metal powder material has conductivity generally, and the performance makes the metal powder material commonly used in daily life. However, in many other applications, only good strength, hardness, toughness and no conductivity are required, and thus surface insulation is necessary. Common processing methods are to coat a film on the surface of the powder, and technologies for realizing the film coating on the surface of the powder include a chemical vapor deposition method, a physical vapor deposition method and an electrochemical method. The chemical vapor deposition method generally has higher temperature requirement and is not easy to control reaction products; the electrochemical method is relatively easy to prepare, but is easy to pollute the powder and cannot separate impurities. The physical vapor deposition method can prepare coating powder under the condition of lower temperature, and mainly comprises a multi-arc ion plating method and a magnetron sputtering method, wherein the magnetron sputtering method has higher plating film purity and better binding property.
At present, the types of the coating materials can be classified into organic materials and inorganic materials. The organic coating is generally made of high molecular polymer, and the coating is easy to realize, but the high polymer is generally not resistant to high temperature, and is easy to decompose when used in a high-temperature environment, so that the insulation effect is poor. The inorganic coating is typically an oxide coating. The metal oxide has higher heat-resistant temperature, can meet the high-temperature use environment, has very high resistivity, and is an excellent insulating coating agent. Patent CN112735722a discloses coating magnetic powder with some oxide mixtures, but it is difficult to ensure uniformity and compactness of coating. While patent CN108597711B discloses a method for coating a layer of Al2O3 insulating layer on the surface of a metal soft magnetic powder by adopting a similar hydrothermal method, wherein Al2O3 is a better insulating coating agent, but the hydrothermal method cannot be applied to large-scale production and has a certain potential safety hazard,
disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method of a metal powder surface insulating layer, which comprises the steps of firstly preprocessing powder to be processed, then plating a layer of metal simple substance film on the powder surface by using a magnetron sputtering method, then forming a uniform and compact metal coating layer on the surface by high-temperature treatment, and finally forming a metal oxide insulating layer with tight combination and good thermal stability by oxidation treatment of the coating layer.
In order to achieve the above purpose, the present invention provides the following technical solutions: a method for preparing a metal powder surface insulation layer, the method comprising the following steps:
s1: immersing the powder into ethanol solution for ultrasonic excitation, immersing into deionized water for ultrasonic cleaning, and then placing into a vacuum drying oven for drying treatment;
s2: placing the pretreated powder into a coated powder preparation box body, mounting the coated powder on a carrying disc, then mounting a target sputtering source, closing a magnetron sputtering chamber, and starting a vacuum pumping system to perform vacuum extraction;
s3: when the vacuum draw reaches the background vacuum of 8.0X10 -4 After Pa, opening an argon valve, introducing argon, then opening a target sputtering power supply, and pre-sputtering the target to remove impurities attached to the surface of the target; then starting an ultrasonic vibration motor, coating the powder, closing the power of a target sputtering source after the powder coating on the conveyor belt is completed, closing the ultrasonic vibration motor, and conveying the powderSending the powder into a powder collecting box;
s4: placing the coated powder into a crucible, placing the crucible into a high-temperature atmosphere furnace, sealing the furnace, vacuumizing, filling inert gas, and performing high-temperature treatment;
s5: cooling after the heat preservation of the high-temperature atmosphere furnace is finished, opening a gas outlet of the furnace to enable inert gas to escape, and carrying out surface oxidation treatment after air enters;
s6: and taking out the powder after the temperature of the high-temperature atmosphere furnace is reduced to room temperature, and sieving.
As a further improvement of the invention, the ultrasonic cleaning time of the ethanol solution in the S1 is 5-10 min, the ultrasonic cleaning time of the deionized water is 10-20 min, the drying temperature is 60-100 ℃ and the drying time is 60-120 min.
As a further improvement of the invention, the flow range of the argon gas introduced in the S3 is 30-50 sccm, the pre-sputtering time range of the target material is 10-30 min, and the film coating time range of the powder is 30-60 min.
As a further improvement of the invention, the high temperature treatment temperature in the S4 is 600-1200 ℃, and the temperature rising rate is 6-10 ℃/min. The high temperature treatment time is in the range of 0.5-4h.
As a further improvement of the invention, the temperature in the S5 is reduced to 500-700 ℃.
As a further improvement of the invention, the temperature of the surface oxidation treatment of the powder in the step S5 is 600 ℃ for heat preservation, and the time of the oxidation treatment is 1h.
As a further improvement of the present invention, the inert gas is nitrogen or argon.
As a further improvement of the invention, the included angle between the target sputtering source and the carrying disc is 40-50 degrees.
As a further improvement of the invention, in the step S3, after the air pressure in the sputtering chamber is lower than 0.5-1 Pa, the pre-pumping valve is closed, the pre-stage valve is opened in sequence, and the molecular pump and the gate valve are used for pumping high vacuum.
The invention has the beneficial effects that:
(1) The method comprises the steps of preprocessing powder to be processed, plating a layer of metal simple substance film on the surface of the powder by using a magnetron sputtering method, forming a uniform and compact metal coating layer on the surface by high-temperature treatment, and finally forming a metal oxide insulating layer with tight combination and good thermal stability by oxidizing the coating layer.
(2) The invention can keep the surface coating of the powder at higher purity by continuous magnetron sputtering coating, and has no other impurities.
(3) The invention can solve the defect of uneven coating of the powder surface coating by high-temperature treatment, so that the coating on the powder surface forms a uniform and compact protective layer.
(4) The invention carries out oxidation treatment after the powder surface layer is coated with the uniform and compact metal simple substance protective layer, thereby not only achieving the effect of forming a metal oxidation insulating layer, but also effectively avoiding the inner layer metal powder from being oxidized, carrying out continuous coating powder production, and being safe and reliable.
Drawings
FIG. 1 is a schematic SEM diagram of a first embodiment of the invention before and after coating;
fig. 2 is a schematic SEM of the second embodiment of the invention before and after coating.
Detailed Description
The invention will now be described in further detail with reference to the drawings and examples. Wherein like parts are designated by like reference numerals. It should be noted that the words "front", "back", "left", "right", "upper" and "lower" used in the following description refer to directions in the drawings, and the words "bottom" and "top", "inner" and "outer" refer to directions toward or away from, respectively, the geometric center of a particular component.
Referring to fig. 1-2, a method for preparing a metal powder surface insulation layer is characterized in that: the method comprises the following steps:
s1: immersing the powder into ethanol solution for ultrasonic excitation, immersing into deionized water for ultrasonic cleaning, and then placing into a vacuum drying oven for drying treatment;
s2: placing the pretreated powder into a coated powder preparation box body, mounting the coated powder on a carrying disc, then mounting a target sputtering source (whether the number is required or not), closing a magnetron sputtering chamber, and starting a vacuum pumping system to perform vacuum extraction;
s3: when the vacuum draw reaches the background vacuum of 8.0X10 -4 After Pa, opening an argon valve, introducing argon, then opening a target sputtering power supply, and pre-sputtering the target to remove impurities attached to the surface of the target; then starting an ultrasonic vibration motor, coating the powder, closing the power of a target sputtering source after the powder coating on the conveyor belt is completed, closing the ultrasonic vibration motor, and conveying the powder to a powder collecting box;
s4: placing the coated powder into a crucible, placing the crucible into a high-temperature atmosphere furnace, sealing the furnace, vacuumizing, filling inert gas, and performing high-temperature treatment;
s5: cooling after the heat preservation of the high-temperature atmosphere furnace is finished, opening a gas outlet of the furnace to enable inert gas to escape, and carrying out surface oxidation treatment after air enters;
s6: and taking out the powder after the temperature of the high-temperature atmosphere furnace is reduced to room temperature, and sieving.
Referring to fig. 1-2, the ultrasonic cleaning time of the ethanol solution in S1 ranges from 5 to 10min, the ultrasonic cleaning time of the deionized water ranges from 10 to 20min, the drying temperature ranges from 60 to 100 ℃ and the drying time ranges from 60 to 120min.
Referring to fig. 1-2, the flow rate of argon introduced in the step S3 ranges from 30 sccm to 50sccm, the pre-sputtering time for the target is 10min to 30min, and the film coating time for the powder is 30min to 60min.
Referring to fig. 1-2, the high temperature treatment temperature in the S4 is 600-1200 ℃, and the temperature rising rate is 6-10 ℃/min. The high temperature treatment time is in the range of 0.5-4h.
Referring to fig. 1-2, the temperature is reduced to 500-700 ℃ in the step S5.
Referring to fig. 1-2, the temperature of the surface oxidation treatment of the powder in S5 is 600 ℃ and the time of the oxidation treatment is 1h.
Referring to fig. 1-2, the inert gas is nitrogen or argon.
Referring to fig. 1-2, the included angle between the target sputtering source and the carrying disc ranges from 40 degrees to 50 degrees.
Referring to fig. 1-2, in the step S3, after the air pressure in the sputtering chamber is lower than 0.5-1 Pa, the pre-pumping valve is closed, the pre-stage valve is opened in sequence, and the molecular pump and the gate valve are used for pumping high vacuum.
First embodiment: irregular copper powder with a median diameter of 25 μm was selected as the subject.
Working principle: immersing the irregular copper powder with the median diameter of 25 mu m in ethanol solution for ultrasonic cleaning for 5min, immersing in deionized water for ultrasonic cleaning for 10min, and then placing in a vacuum oven for drying treatment at the temperature of 80 ℃ for 30min. And placing the pretreated powder into a coated powder preparation box body, mounting the coated powder on a carrying disc, then mounting an aluminum target, closing a magnetron sputtering chamber, and starting a vacuum pumping system to perform vacuum extraction. The vacuum reached background vacuum 8.0X10 - 4 After Pa, opening an argon valve, introducing 40sccm argon, then opening a sputtering power supply of the target, and pre-sputtering the target for 20min to remove impurities attached to the surface of the target; then starting an ultrasonic vibration motor, and coating the powder for 40min; after the powder coating on the conveyor belt is completed, the power of the sputtering source of the target is closed, the ultrasonic vibration motor is closed, and the powder is conveyed to the powder collecting box. And placing the coated powder into a crucible and placing the crucible into a high-temperature atmosphere furnace. And (5) vacuumizing after sealing the furnace, and filling a small amount of argon. Then high temperature treatment is carried out, the high temperature treatment temperature is 700 ℃, and the temperature rising rate is 8 ℃/min. The incubation time was 2h. And cooling the gas to 600 ℃ after heat preservation, opening a gas outlet of the furnace, allowing argon to escape, allowing air to enter, preserving heat for 1h, and performing surface oxidation treatment. And taking out the powder after the temperature is reduced to room temperature, and sieving to obtain the powder coated with the Al2O3 insulating layer.
Specific embodiment II: referring to FIG. 2, a spherical titanium alloy powder having a median diameter of 20 μm was selected as an experimental subject.
Working principle: immersing spherical titanium alloy powder with the median diameter of 20 mu m in ethanol solution for ultrasonic cleaning for 10min, and immersing in deionized waterUltrasonic cleaning for 15min, and then placing into a vacuum oven for drying treatment, wherein the drying temperature is 80 ℃ and the drying time is 30min. And placing the pretreated powder into a coated powder preparation box body, mounting the coated powder on a carrying disc, then mounting an aluminum target, closing a magnetron sputtering chamber, and starting a vacuum pumping system to perform vacuum extraction. The vacuum reached background vacuum 8.0X10 -4 After Pa, opening an argon valve, introducing 40sccm argon, then opening a sputtering power supply of the target, and pre-sputtering the target for 20min to remove impurities attached to the surface of the target; then starting an ultrasonic vibration motor, and coating the powder for 50min; after the powder coating on the conveyor belt is completed, the power of the sputtering source of the target is closed, the ultrasonic vibration motor is closed, and the powder is conveyed to the powder collecting box. And placing the coated powder into a crucible and placing the crucible into a high-temperature atmosphere furnace. The furnace was sealed and then evacuated and then purged with a small amount of argon. Then high temperature treatment is carried out, the high temperature treatment temperature is 750 ℃, and the temperature rising rate is 10 ℃/min. The incubation time was 2h. Cooling the gas to 600 ℃ after heat preservation, opening an air outlet of the furnace to enable argon to escape, allowing air to enter, preserving heat for 1h, carrying out surface oxidation, taking out powder after the temperature is reduced to room temperature, and sieving to obtain powder coated with the Al2O3 insulating layer.
The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (9)
1. A preparation method of a metal powder surface insulating layer is characterized by comprising the following steps: the method comprises the following steps:
s1: immersing the powder into ethanol solution for ultrasonic excitation, immersing into deionized water for ultrasonic cleaning, and then placing into a vacuum drying oven for drying treatment;
s2: placing the pretreated powder into a coated powder preparation box body, mounting the coated powder on a carrying disc, then mounting a target sputtering source, closing a magnetron sputtering chamber, and starting a vacuum pumping system to perform vacuum extraction;
s3: when the vacuum extraction reaches the background vacuum of 8.0 XPa, opening an argon valve, introducing argon, then opening a target sputtering power supply, and pre-sputtering the target to remove impurities attached to the surface of the target; then starting an ultrasonic vibration motor, coating the powder, closing the power of a target sputtering source after the powder coating on the conveyor belt is completed, closing the ultrasonic vibration motor, and conveying the powder to a powder collecting box;
s4: placing the coated powder into a crucible, placing the crucible into a high-temperature atmosphere furnace, sealing the furnace, vacuumizing, filling inert gas, and performing high-temperature treatment;
s5: cooling after the heat preservation of the high-temperature atmosphere furnace is finished, opening a gas outlet of the furnace to enable inert gas to escape, and carrying out surface oxidation treatment after air enters;
s6: and taking out the powder after the temperature of the high-temperature atmosphere furnace is reduced to room temperature, and sieving.
2. The method for preparing a metal powder surface insulation layer according to claim 1, wherein: the ultrasonic cleaning time range of the ethanol solution in the step S1 is 5-10 min, the ultrasonic cleaning time range of the deionized water is 10-20 min, the drying temperature range is 60-100 ℃, and the drying time is 60-120 min.
3. The method for preparing a metal powder surface insulation layer according to claim 2, characterized in that: and the flow range of the argon gas introduced in the step S3 is 30-50 sccm, the pre-sputtering time range of the target material is 10-30 min, and the film coating time range of the powder is 30-60 min.
4. The method for preparing a metal powder surface insulation layer according to claim 1, wherein: the high temperature treatment temperature in the step S4 ranges from 600 ℃ to 1200 ℃ and the temperature rising rate ranges from 6 ℃ to 10 ℃/min. The high temperature treatment time is in the range of 0.5-4h.
5. The method for preparing a metal powder surface insulation layer according to claim 1, wherein: and (5) cooling to 500-700 ℃ in the step (S5).
6. The method for preparing a metal powder surface insulation layer according to claim 1, wherein: and (5) carrying out heat preservation at 600 ℃ on the surface of the powder in the step (S5), wherein the time of the oxidation treatment is 1h.
7. The method for preparing a metal powder surface insulation layer according to claim 1, wherein: the inert gas is nitrogen or argon.
8. The method for preparing a metal powder surface insulation layer according to claim 1, wherein: the included angle between the target sputtering source and the carrying disc is 40-50 degrees.
9. The method for preparing a metal powder surface insulation layer according to claim 1, wherein: and in the step S3, after the air pressure in the sputtering chamber is lower than 0.5-1 Pa, closing the pre-pumping valve, and sequentially opening the backing valve, and pumping high vacuum by the molecular pump and the gate valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311566707.4A CN117512516A (en) | 2023-11-22 | 2023-11-22 | Preparation method of metal powder surface insulation layer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311566707.4A CN117512516A (en) | 2023-11-22 | 2023-11-22 | Preparation method of metal powder surface insulation layer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117512516A true CN117512516A (en) | 2024-02-06 |
Family
ID=89760464
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311566707.4A Pending CN117512516A (en) | 2023-11-22 | 2023-11-22 | Preparation method of metal powder surface insulation layer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117512516A (en) |
-
2023
- 2023-11-22 CN CN202311566707.4A patent/CN117512516A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP3056585B1 (en) | A method of disposing an aluminum coating on nd-fe-b permanent magnets | |
| US8070926B2 (en) | Multi-chamber workpiece processing | |
| JPH0338339B2 (en) | ||
| CN100569991C (en) | A kind of preparation method of titanium surface black oxidation titanium film | |
| CN102787300A (en) | Cr/CrAlN gradient coating technology of supercritical water-cooled reactor fuel can surface | |
| EP3056584B1 (en) | Method for making nd-fe-b permanent magnets with anti-corrosive composite coating | |
| CN111224121A (en) | In-situ preparation method of surface composite modified layer of stainless steel bipolar plate of proton exchange membrane fuel cell | |
| CN108130515A (en) | A kind of preparation method of long-life thermal barrier coating | |
| CN117512516A (en) | Preparation method of metal powder surface insulation layer | |
| JP4694771B2 (en) | Pump and pump member manufacturing method | |
| CN112374911A (en) | Surface treatment method of graphite substrate and preparation method of TaC coating | |
| CN112097523A (en) | Atmosphere box type sintering furnace for production of mobile phone back plate | |
| CN112159951B (en) | Preparation process of water erosion resistant layer of turbine titanium alloy blade | |
| CN113005406B (en) | Preparation method of niobium-tin film | |
| US20120171501A1 (en) | Process for surface treating magnesium alloy and article made with same | |
| CN112323066B (en) | Preparation method of diffusion barrier layer suitable for large-scale component | |
| CN111850456A (en) | Titanium alloy segmented vacuum rapid nitriding method and device | |
| JP2022104855A (en) | Corrosion-resistant neodymium iron-boron magnet, surface treatment method, and usage of hydroxyl group compound | |
| CN109576637B (en) | Carburizing method for hard alloy | |
| US8609241B2 (en) | Coated article and method of making the same | |
| CN114134456A (en) | Magnetron sputtering preparation method of Cr coating of zirconium alloy cladding | |
| CN106480402A (en) | Film formation device and film build method | |
| CN111575645A (en) | Oxidation-resistant coating containing aluminum storage layer and preparation method thereof | |
| CN110565061A (en) | environment-friendly process for directly plating easy-to-oxidize metal film | |
| JPS6362862A (en) | Ceramic coated ti and ti alloy product and its production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |